Synthesis and Crystal Structure of α-Mo4XS3(μ-dtp)3(dtp)3 (X=0.6S + 0.4O)

The title compound (Mo4XS15P6O12C24H30), α-Mo4XS3(μ-dtp)3(dtp)3 (X=0.6S+0.4O; dtp=-S2P[OEt]2), isolated as a prismatic black crystal, was prepared from ethanolic solution of Mo(CO)6, MoCl5 and P2S5. It crystallizes in triclinic system, space group P with a=14.031(4), b=13.372(2), c=16.270(8)(A), α=92.15(2), β = 72.91(3), γ = 95.20(2)°, V = 2905.4(2)(A)3, Z = 2, Dc = 1.82 g/cm3, Mr=1598.93, F(000)=1564.8, λ=0.71069(A)(MoKα), μ=1.584 mm-1. The final R=0.058, Rw=0.057 for 5016 observed reflections with I≥3.0σ(I). The structure analysis reveals that the title compound has a [Mo4XS3] core, belonging to the cubane-type tetranuclear molybdenum clusters family, with one of its four μ3-caps being statistically occupied by S and O. Three dtp ligands chelated three μ-X capped Mo atoms as terminal ligands, while another three dtp bridged these three Mo atoms and the fourth one, forming an α-type cluster compound.     

Synthesis and Crystal Structure of MnSm_4(SiO_4)_3O

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＭｎＳｍ_４（ＳｉＯ_４）_３Ｏ￥ＣｈｉＬｉ－Ｓｈｅｎｇ；ＤｅｎｇＳｈｕｉ－Ｑｕａｎ；ＺｈｕａｎｇＨｏｎｇ－Ｈｕｉ；ＨｕａｎｇＪｉｎ－Ｓｈｕｎ；（ＳｔａｔｅＨｅｙｌａｂｏｒａｔｏｒｙｏｆＳｔｒ?..     

Synthesis and Crystal Structure of Co(C_6NO_2H_4)_3. H_2O

1INTRoDUCTIONAlotofresultsoncobaltcomplexstructureshavebeenreportedforseveraldecades.Theinterestofresearchinthisfieldhasneverbeenreducedbecausethecobaltcomplexesplayaveryimportantroleinthelifescienceandcatalysis,etc[1-6).WereportherethesynthesisandstructureofcomplexCo(C,NO,H'),.H,O.2EXPERIMENTALAllreagentsandsolventsusedareofARgradefromcommericalsourceswithoutfurtherpurification.ThetitlecompoundCo(C,NO,H,),.H,Owassynthesizedbythefollowingmethod.When2.4g(ca.1mmol)ofCoCl2.6H2Ow…     

Syntheses and Crystal Structures of Molybdenum-Sulfur Clusters Mo_3S_4 (dtp)_3(o-CH_3OC_6H_4COO)(Py) and Mo_3S_4 (dtp)_3(p-HOC_6H_4COO)(DMF)·EtOH

1 INTRODUCTION Recent years have seen a drastic increase of compounds containing the Mo3S4 core. A major synthetic route to these compounds is by the reaction of the aqua ion [Mo3S4(H2O)9]4+ with different kinds of ligands replacing some or all of the water molecules. In this way, Mo3S4(dtp)4(H2O), which was synthesized by the spontaneous- assembly method in 1986[1] and its structural characterization and chemical reactivity have been well recognized [2], can be rationally synthesize…     

Synthesis and Crystal Structure of Ho_4S_3Si_2O_7

1 INTRODUCTION Halide fluxes are excellent media for growing single crystals of chalcogenides[1~5]. On our research in the Ln-Cu-Zn-Se system to find new phases and to search for potential infrared ceramic materials, two new compounds, KHo2CuSe4 and KEr2CuSe4, were synthesized from the reaction of the precursor with KCl flux[6]. In an attempt to synthesize the homologous sulfide by the same method using KBr as flux in a sealed evacuated quartz tube, single crystals of Ho4S3Si2O7 w…     

Synthesis and Crystal Structure of μ_(1,1,3) Formic Bridging 3D Microporous Ni(II) Complex

A μ1,1,3 formic bridging Ni2+ complex [Ni3(HCOO)6·H2O]]n 1 has been synthesi- zed under hydrothermal conditions. The single-crystal X-ray diffraction analysis shows that 1 exhibits a 3D open microporous tube formed by covalent and coordination bonds. Complex 1 crystallizes in the monoclinic system, space group P21/c with a = 11.1487(13), b = 9.7763(11), c =17.9685(17) , β = 126.948(6)o, C6H6Ni3O13, Mr = 462.02, V = 1565.2(3) 3, Z = 4, Dc = 1.961 g/cm3, μ = 3.630 mm-1, F(000) = 917.7, Rint = 0.0234, the final R = 0.0234 and wR = 0.0734 for 3469 observed reflections (I>2σ(I)).     

Synthesis and Structure of μ-Peroxo-bis(4-bromophenoxotri-p-tolylantimony)

-Peroxo-bis(4-bromophenoxotri-p-tolylantimony) was synthesized by reacting 4-bromophenol with tri-p-tolylstibine in the presence of hydrogen peroxide. According to X-ray diffraction data, the Sb atoms have trigonal bipyramidal coordination. In the centrosymmetric molecule, the two Sb atoms are joined via bridging peroxo group disordered over two sites. The Sb–O(1,2') bond lengths are equal to 1.999(6) and 2.03(1) Å, the Sb···O(2,1') distances are equal to 2.605(9) and 2.626(5) Å, respectively. The lengths of the terminal Sb–O(3) bonds are 2.093(3) Å.     

Synthesis and Crystal Structure of a Cyano-bridged Bimetallic Complex:[NdFe(CN)_6(DMF)_4(H_2O)_3]H_2O

1 INTRODUCTION In recent years, cyano-bridged heterometallic coordination compounds have inspired remarkable attention due to their rich and interesting structures and magnetic behaviors. However, these studies were mainly focused on the transition metals. Although several unusual cyanide bridging lanthanide-transition metal complexes have been re- ported[1～6], this field continuously possesses tre- mendous researching potentialities. As regardsPrussian Blue lanthanide complex, divers…     

Synthesis and Crystal Structure of (L)_2W(CO)_4·CH_3COCH_3 (L=1-Phenacylimidazole)

1 INTRODUCTION Due to their variability in binding modes, five- membered heterocyclic ligands such as pyrazole[1] and 1,2,4-triazole[2] have been drawn much attention. Consequently, there are numerous reports on their derivatives. Imidazoles resemble pyrazoles, and they are isomeric five-membered heterocyclic molecules containing two nitrogen atoms. Furthermore, imida- zole is also a ring component of adenine and purine, one of the most versatile binding sites in biological systems, so th…     

Synthesis and Crystal Structure of Triacetyltribenzyl-Hexaazaisowurtzitane (TATBIW·0.5 H)_2O)

The hexanitro hexaaza isowurtzitane (HNIW) (2, 4, 6, 8, 10, 12-hexanitro-2, 4, 6, 8, 10,12-hexaazatetracyclo-[5.5.0.05,9.03,11]-dodecane), more commonly called CL-20, be-longs to the family of high energetic dense caged nitramines. It was first synthesized byA.T.Nielsen in 19871. HNIW is superior to HMX with respect to density, velocity,detonation pressure and enthalpy of formation. Based on cylinder expansion andtantalume plate acceleration experiments, the HNIW was found to be appr…     

Synthesis and Crystal Structure of {[Mn(H_2O)_4(3,3''''-?azpy)](3, 3''''-azpy)_3(PF_6)_2}_n

1 INTRODUCTION During the past few years, many one-, two- and three-dimensional coordination polymers have been generated from transition metal templates with rigid and flexible pyridyl-containing bidentate or multidentate spacers[1, 2]. Although in the past few years, increasing interest has been given to the coordination polymer of 4, 4?azobispyridine[3, 4] and some 3, 3?azobispyridine complexes[5, 6] were repor- ted three decades ago, no crystal structure of 3, 3?azpy complex has been…     

Synthesis and Crystal Structure of a Heteronuclear Erbium and Yttrium Complex with Proline: [ErY(pro)_6(H_2O)_6] (ClO_4)_6

1INTRODUCTIONThephysiologicaleffectofrareearthionshasarousedgreatattentionrecent-lya'"-Aminoacids,assmallbio-moleculeswithspeialfunctions,existinplasmainhighconcentrations(3),sothestudyontheinteractionsbetweenrareearthionsandaminoacidsmayshedsomelightsonthephysiologicaleffectofrareearthsion.Inthepastfewyears,about4orareearthcomplexeswithaminoacidswereStructurallycharacterndt'3.Amongthemsevenaretheprolinecomplexes.Intheseprolinecom.plexes,molarratioofmetal(M)andproline(L)M:L=1:1complexis…     

STUDY OF ELECTROCHEMISTRY OF TETRANUCLEAR MOLYB-DENUM CLUSTER COMPOUND [Mo_4S_4(μ-dtp)_2(dtp)_4]

<正> The electrochemical behavior of tetranuclear molybdenum cluster [Mo4S4 (μ-dtp)2 (dtp)43 (1) (dtp = S2P (OEt)2) has been investigated by cyclic voltammetry, potentiotatic polarization measurement, controlled potential coulometry and pulse polarography. It is demonstrated that the compound undergoes two consecutive near reversible one-electron reductions at 0. 01V and -0. 77V , respectively and a near reversible one-electron oxidation at 1. 01V with scan rates from 25mV/sec to 1V/sec in cyclic voltammetric measurements. The cluster compound displays three redox processes, indicating its high structural stability.     

Synthesis and Crystal Structure of 〔Co_3(CO)_9(μ_3-C)C(O)OCH_2〕_2

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Synthesis and Crystal Structure of Ni_3(admt)_6(NCS)_6·C_2H_5OH·2H_2O

1　INTRODUCTIONCoordination compounds with 1 ,2 ,4 triazole as a ligand have interesting fea tures,notonly because ofthe very interesting magnetic propertiesofthese complex es,but also because ofrich modes ofcoordination〔1〕.Particularly,the coordinationbehavioroftriazoletowardsa numberoftransition metalthiocyanatesshowsremark abledifferences〔2 - 6〕.On unsubstitution at N4 ,thetriazole ring hasmonodentate,1 ,2 and 2 ,4 bridging forms.These three modes were all observed in the Ni( II)…     

Synthesis and Crystal Structure of [Cu(acac)(Hdmpz)_3]Br.EtOH

1 INTRODUCTION Diazoles have both a pyridine-type nitrogen and a pyrrole-type nitrogen (imino group), so they can act as bifunctional groups to coordinate with many metal ions or Lewis acids giving a variety of products[1, 2]. Recently researches on the pyrazole ligand have been focused on the following three sections. (i) The first is that the ligand acts as a bridged ligand and coordinates to metal forming di- and polynuclear complexes. Such system arouses much interest mainly because o…     

Synthesis and Crystal Structure of ｛( P Ph_3)_2 Cl Ru( μ- Cl) Ru( P Ph_3) B_(10)H_7〔 O C H( C H_3)_2〕_3｝·0 .4( H_2O)

１　ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅｆｉｒｓｔｐｏｌｙｈｅｄｒａｌｒｕｔｈｅｎａｂｏｒａｎｅｉｓｓｔｒｕｃｔｕｒａｌｌｙｔｙｐｉｆｉｅｄｂｙｔｈｅｃｏｍｐｏｕｎｄ〔（ＰＰｈ３）２ＲｕＢ１０Ｈ８（ＯＥｔ）２〕ｉｎ１９８４〔１〕,ｗｈｉｃｈｉｓｏｂｔａｉｎｅｄｉｎ４０％ｙｉｅｌｄｂｙｔｈｅｒｅａｃｔｉｏｎｏｆｔｈｅｃｌｏｓｏｄｅｃａｂｏｒａｎｅａｎｉｏｎＢ１０Ｈ１０２－ｗｉｔｈ〔ＲｕＣｌ２（ＰＰｈ３）３〕ｉｎｅｔｈａｎｏｌ／ｃｈｌｏｒｏｆｏｒｍｓｏｌｕｔｉｏｎ．Ｒｅｓｅａｒｃｈｅｒｓｈａｖｅｓｙ…     

Synthesis and Crystal Structure of (C_6N_3H_(18))_2Ti_4O_4(C_2O_4)_7·4H_2O

1 INTRODUCTION The open-framework inorganic materials have been synthesized before the early 1980s[1]. Parti- cularly, metal phosphates have been investigated widely during the past few years[2, 3]. In recent years, considerable efforts have been devote…     

Synthesis and Crystal Structure of (C6N3H18)2Ti4O4(C2O4)7·4H2O

The title compound (C6N3H18)2Ti4O4(C2O4)7(4H2O 1 (C13H22N3O18Ti2, Mr = 604.14) was synthesized by the reaction of Ti(SO4)2, H2C2O4(2H2O and N-(2-ammonioethyl)- piperazinium (AEPP) in aqueous solution. The single-crystal X-ray analysis has revealed that 1 crystallizes in the triclinic system, space group Pī with a = 9.1437(6), b = 11.4991(10), c = 11.6975(8)A, α = 96.2915(18), β = 107.998(3), γ = 104.276(4)°, V = 1110.35(14)A3, Z = 2, Dc = 1.807 g/cm3, F(000) = 618, μ = 0.815 mm－1, the final R = 0.0463 and wR = 0.1264 for 3718 observed reflections with I > 2σ(I). X-ray crystal-structure analysis suggests that compound 1 consists of [Ti4O4(C2O4)7]6－ anion and two protonated N-(2-ammonioethyl)piperazinium cations. The anions are linked into an infinite chain through Ti4O4(C2O4)8 by sharing the oxalates as bridging ligands.